CN102386378A - Preparation method for electrode slurry of lithium ion batteries - Google Patents
Preparation method for electrode slurry of lithium ion batteries Download PDFInfo
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- CN102386378A CN102386378A CN2011102680400A CN201110268040A CN102386378A CN 102386378 A CN102386378 A CN 102386378A CN 2011102680400 A CN2011102680400 A CN 2011102680400A CN 201110268040 A CN201110268040 A CN 201110268040A CN 102386378 A CN102386378 A CN 102386378A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the manufacture field of lithium ion batteries, and particularly relates to a preparation method for electrode slurry of the lithium ion batteries, which includes premixing and stirring. During premixing, fog state premixing is conducted on both liquid materials and powder materials simultaneously in a mixing cavity in an atomizing mode. During stirring, mixture obtained by premixing is mechanically stirred to prepare the electrode slurry. Due to the fact that particles adopt the atomizing and are miniaturized, wetting of the powder materials by solvent can be improved, dispersibility is improved, more even electrode slurry can be obtained during short time in the following conventional mechanical stirring, uniformity of the slurry can be effectively improved, and slurrying efficiency is greatly improved.
Description
Technical field
The invention belongs to lithium ion battery and make the field, more particularly, the present invention relates to a kind of preparation method of lithium ion battery electrode sizing agent.
Background technology
Because lithium ion battery has that energy density height, reliability are high, processability is good and advantage such as non-environmental-pollution, is widely used at present like all kinds of portable electric appts such as smart mobile phone, notebook, panel computers.
Lithium ion battery generally comprises positive plate, negative plate, is interval in the barrier film between positive plate and the negative plate.Positive plate comprises plus plate current-collecting body and is distributed in the anodal diaphragm on the plus plate current-collecting body that negative plate comprises negative current collector and is distributed in the cathode membrane on the negative current collector.Preparation is during electrode plates, with active material (like graphite, cobalt acid lithium; LiMn2O4s etc.), conductive agent (like acetylene black, Super-P, CNT, carbon fiber etc.), bonding agent (like Kynoar, PVP, sodium carboxymethylcellulose, SBR emulsion etc.) and solvent (like N-methyl pyrrolidone, water etc.) etc. mix and process electrode slurry; Common pulp preparation mode is to use two planetary dispersing apparatus; Bonding agent is dissolved in the solvent, adds conductive agent then and disperse, add active material at last and additive further disperses; Obtain final electrode slurry; Again it is coated in collection liquid surface on request, carries out drying then, obtain battery pole piece.
Wherein the performance of electrode slurry is to lithium ion battery performance important influence.If electrode slurry disperses more evenly, can make that electrode impedance everywhere is even, the effect of active material can be brought into play more fully when discharging and recharging, thereby promotes the performance of full battery.
But; In the preparation process of existing pulp of lithium ion battery; Because the difference of each material physicochemical properties like specific area, amphipathic property etc., can produce wetting difficulty in the process that stirs; Particle conglomerations etc. disperse irregular phenomenon, adopt mechanical agitation to be difficult to the effect that reaches desirable merely.In addition, because the wetting difficulty that exists between each material can reach very high viscosity in whipping process, make the load of mixing plant increase greatly, long-term use meeting causes damage to mixing plant.
In view of this, necessaryly provide a kind of and can obtain slurry dispersion effect preferably, can reduce equipment loss and improve the pulp of lithium ion battery preparation method of slurrying efficient.
Summary of the invention
The objective of the invention is to: provide a kind of and can obtain slurry dispersion effect preferably, can reduce equipment loss and improve the pulp of lithium ion battery preparation method of slurrying efficient.
To achieve these goals, the present invention adopts following technical scheme:
A kind of preparation method of lithium ion battery electrode sizing agent,
Premix: in hybrid chamber, adopt spray pattern simultaneously liquid material and powder material to be advanced the mist state premix;
Stir: the mixture behind the premix is carried out mechanical agitation, make electrode slurry.
As a kind of improvement of lithium ion battery electrode sizing agent preparation method of the present invention, liquid material and powder material all adopt spray pattern, and the two mixes under the contact of certain turbulent flow mode.Because powder and solvent have all formed littler particle, can greatly increase the area of the two physics contact,, the two improves the efficient of soaking between the two, and the effect of improvement infiltration when mixing effectively.Owing to improved the problem that material soaks into, in next step mechanical agitation, can obtain electrode slurry more uniformly in the short period of time.
As a kind of improvement of lithium ion battery electrode sizing agent preparation method of the present invention, described various powders can spray separately simultaneously, also can various powders be pre-mixed even back and spray.
As a kind of improvement of lithium ion battery electrode sizing agent preparation method of the present invention, described powder material comprises active material powder, conductive agent powder, bonding agent powder and additive agent powder, or wherein at least a.
A kind of improvement as lithium ion battery electrode sizing agent preparation method of the present invention; Described liquid material is any one or the two or more combination in water, alcohol, acetone, N-methyl pyrrolidone, dimethyl formamide, dimethylacetylamide or the dimethyl sulfoxide (DMSO), or is the solution of one or more bonding agents.
Can change according to the needs of actual process.In order to improve the processing characteristics in the battery manufacture process, improve the electrical property or the security performance of battery, can in liquid material, add proper additive in advance.
A kind of improvement as lithium ion battery electrode sizing agent preparation method of the present invention; Before liquid material spraying and powder material sprinkling; Can also carry out the pre-treatment of physics modes such as heat, electricity, magnetic to liquid or powder; Improving powder or solvent physicochemical properties, thereby improve electrode slurry processing characteristics or final battery performance at aspects such as composition mode, surface texture, crystal orientation or reactivities.
As a kind of improvement of lithium ion battery electrode sizing agent preparation method of the present invention, the average diameter of the mist attitude drop that liquid material forms is between 1～500 micron.Prove that the average diameter of particle is difficult to form the mist attitude during greater than 500 microns, is easy to form big drop through test of many times.
As a kind of improvement of lithium ion battery electrode sizing agent preparation method of the present invention, the average grain diameter of the particle that powder material forms is between 0.1～50 micron.
As a kind of improvement of lithium ion battery electrode sizing agent preparation method of the present invention, the weight proportion of liquid material and powder material is between 98: 2～20: 80.If the proportioning of powder material is excessive, solid content is higher, can make flowing of slurry slow, is unfavorable for collecting, and production efficiency is low.
As a kind of improvement of lithium ion battery electrode sizing agent preparation method of the present invention, said liquids materials flow can adopt the turbulent flow mode to contact with powder material stream, like collision type contact, spiral vortex type contact or other turbulent flow modes.Adopt the turbulent flow mode to contact and to let the liquids materials flow produce as much as possible the contact at short notice with powder material stream; Increase the contact area and the contact probability of liquid material and powder material; Improve the efficient of soaking between the two effectively, and improve the effect of soaking into.
With respect to prior art, the present invention has the following advantages at least:
The first, through premix that liquid material and powder material are sprayed, increased effective contact area between the two, can improve infiltration between the two effectively.
The second, liquid material and powder material are accomplished premixed within a short period of time, can obviously reduce the time of stirring, enhance productivity.
The 3rd, because the improvement of soaking into, can make that each component is disperseed more even in the electrode slurry between the two.
The 4th, in the identical solid-liquid mixing system, because uniformity is good more, its viscosity can be low more.Follow-up churned mechanically resistance descends significantly, can reduce follow-up churned mechanically equipment loss effectively.
Description of drawings
Fig. 1 is the viscosity change curve during with the embodiment 1 making slurry of spraying premix mode of the present invention for the Comparative Examples 1 that adopts common alr mode and graphite and hydromining.
Distribution of particle sizes curve when Fig. 2 adopts the embodiment 2 making slurries of spraying premix mode of the present invention for the Comparative Examples 2 that adopts common alr mode and nano carbon black and CMC solution.
Distribution of particle sizes curve when Fig. 3 adopts the embodiment 3 of spraying premix mode of the present invention to make slurry for the Comparative Examples 3 that adopts common alr mode with graphite powder, carbon black powder and CMC solution.
Fig. 4 is for to be pre-mixed NMP and CMC solution, adopts the mixed solution of graphite powder, carbon black powder, NMP and CMC to adopt the embodiment 4 of spraying premix mode of the present invention then and the distribution of particle sizes curve when adopting the Comparative Examples 4 of common alr mode to make slurries.
Distribution of particle sizes curve when Fig. 5 adopts the embodiment 5 of spraying premix mode of the present invention for the heat treatment solution that adopts graphite powder, carbon black powder and CMC and adopts the Comparative Examples 3 making slurries of common alr mode.
Fig. 6 is for to be dissolved in 1wt% oxalic acid in the PVDF solution in advance, the distribution of particle sizes curve when cobalt acid powder for lithium, carbon black powder adopt the embodiment 6 of spraying premix mode of the present invention with PVDF solution and adopt the Comparative Examples 5 making slurries of common alr mode then.
Embodiment
Goal of the invention of the present invention, technical scheme and technique effect are more clear to be understood in order to make, and below in conjunction with accompanying drawing and embodiment, the present invention is further elaborated.Should be appreciated that the embodiment of describing in this specification only is in order to explain the present invention, is not in order to limit the present invention.
Embodiment 1:
With graphite, CMC solution and water is the feedstock production lithium ion battery cathode slurry.The preparation process is divided two stages.At first be Spray Mixing, graphite powder and CMC solution be injected in the hybrid chamber with the mist attitude respectively simultaneously mix that (powder: weight proportion control liquid) was delivered to the mixture in the collecting chamber in two planetary stirring machines spray volume again according to 60: 40; Second stage is the conventional flow process that stirs, and promptly adds an amount of water by prescription, and high-speed stirred 6 hours obtains final slurry.
In the Spray Mixing stage, the average grain diameter that adopts the droplet distribution recognizer to measure CMC solution droplet is 471.2 microns, and the average grain diameter of graphite dust cloud particle is 24.15 microns.
Comparative Examples 1
Adopt the raw material identical, adopt common alr mode to make slurry with embodiment 1.
Slurry when slurry that obtains when embodiment 1 Spray Mixing is finished and Comparative Examples 1 premix finish compares.Measure two kinds of slurry viscosities with the DV-II of Bookfield company type digital display viscosimeter, Comparative Examples 1 is 6450mPas, and embodiment 1 is 3070mPas.Because viscosity is big more usually, the resistance during stirring is also big more, so the viscosity resistance that Comparative Examples 1 mixing plant receives is much higher than embodiment 1, its machine loading is bigger.In addition, in Comparative Examples 1 and embodiment 1 conventional agitation phases separately, get once appearance at set intervals, measure viscosity respectively with the digital display viscosimeter, the result is as shown in Figure 1.Can find out that under identical mixing time, the viscosity of Comparative Examples 1 all is higher than embodiment 1, up to the stabilized platform district that all gets into viscosity number.Because in the pulp of lithium ion battery system; The low reflection usually of viscosity Dispersion of Particles gets thinner; Then The above results means that embodiment 1 reaches the required mixing time of identical dispersion effect than Comparative Examples 1 still less, adopts mode of the present invention can improve slurrying efficient greatly.
Embodiment 2:
With nanoscale carbon black and CMC solution is feedstock production lithium ion battery conductive agent slurry.The preparation process is divided two stages.At first be Spray Mixing, carbon black powder and CMC solution be injected in the hybrid chamber with the mist attitude respectively simultaneously mix that (powder: weight ratio control liquid) was delivered to the mixture in the collecting chamber in two planetary stirring machines spray volume again according to 2: 98; Second stage is the conventional flow process that stirs, and promptly high-speed stirred is 3 hours, obtains final slurry.
In the Spray Mixing stage, the average grain diameter that adopts the droplet distribution recognizer to measure CMC solution droplet is 94.3 microns, and the average grain diameter of carbon black dust cloud particle is 1.8 microns.
Comparative Examples 2
Adopt the raw material identical, adopt common alr mode to make slurry with embodiment 2.
Get the final slurry of embodiment 2 and Comparative Examples 2 respectively, adopt the Malvern laser particle analyzer to measure the pulp particle degree respectively, the result is as shown in Figure 2.Can find out that the granularity of embodiment 2 is less than Comparative Examples 2, explain under same stirring condition that the slurry of mist attitude premix disperses better effects if.
Embodiment 3:
With graphite, nanoscale carbon black, CMC solution, SBR emulsion and water is the feedstock production lithium ion battery cathode slurry.The preparation process is divided two stages.It at first is Spray Mixing; Graphite powder, carbon black powder and CMC solution is injected in the hybrid chamber with the mist attitude respectively simultaneously mixes; Spray volume was according to 60: 40 (powders: weight ratio control liquid); Wherein graphite is sprayed by two different shower nozzles according to formula rate with hydrocarbon black powder simultaneously, the mixture in the collecting chamber is delivered in two planetary stirring machines again; Second stage is the conventional flow process that stirs, and promptly adds an amount of water and SBR emulsion by prescription, and high-speed stirred 6 hours obtains final slurry.
The average grain diameter that adopts the droplet distribution recognizer to measure the CMC droplet is 449.3 microns, and the average grain diameter of graphite dust cloud particle is 25.21 microns, and the average grain diameter of carbon black dust cloud particle is 1.77 microns;
Comparative Examples 3
Adopt the raw material identical, adopt common alr mode to make slurry with embodiment 3.
Get the final slurry of embodiment 3 and Comparative Examples 3 respectively, adopt the Malvern laser particle analyzer to measure the pulp particle degree respectively, the result is as shown in Figure 3.Can find out that the granularity of embodiment 3 is less than Comparative Examples 3, explain under same stirring condition that the slurry of mist attitude premix disperses better effects if.
Embodiment 4:
Mode according to embodiment 3 prepares lithium ion battery cathode slurry, and that different is the NMP that adds 5wt% in the CMC solution in advance, forms mixed solution.
The average grain diameter that adopts the droplet distribution recognizer to measure CMC mixed solution (adding NMP) droplet is 276.6 microns, and the average grain diameter of graphite dust cloud particle is 26.61 microns, and the average grain diameter of carbon black dust cloud particle is 1.83 microns;
Comparative Examples 4
Adopt the raw material identical, adopt common alr mode to make slurry with embodiment 4.
Get the final slurry of embodiment 4 and Comparative Examples 4 respectively, adopt the Malvern laser particle analyzer to measure the pulp particle degree respectively, the result is as shown in Figure 4.Can find out that the granularity of embodiment 4 is less than Comparative Examples 4, explain under same stirring condition that the slurry of mist attitude premix disperses better effects if.
Embodiment 5:
Mode according to embodiment 3 prepares lithium ion battery cathode slurry, and different is that CMC solution is heated to 45 ℃ in advance, and viscosity is reduced.
The average grain diameter that adopts the droplet distribution recognizer to measure CMC solution droplet is 147.1 microns, and the average grain diameter of graphite dust cloud particle is 24.06 microns, and the average grain diameter of carbon black dust cloud particle is 1.62 microns;
Get the final slurry of embodiment 5 and Comparative Examples 3 respectively, adopt the Malvern laser particle analyzer to measure the pulp particle degree respectively, the result is as shown in Figure 5.Can find out that the granularity of embodiment 5 is less than Comparative Examples 3, explain under same stirring condition that the slurry of mist attitude premix disperses better effects if.
Embodiment 6:
With cobalt acid lithium, nanoscale carbon black, oxalic acid and PVDF solution is the feedstock production lithium ion battery anode glue size.The preparation process is divided two stages.It at first is Spray Mixing; Cobalt acid powder for lithium, carbon black powder and PVDF solution (adding 0.5wt% oxalic acid as additive) are injected in the hybrid chamber simultaneously with the mist attitude respectively and mix; Spray volume was according to 80: 20 (powders: weight ratio control liquid); Wherein cobalt acid lithium is sprayed by two different shower nozzles according to formula rate with hydrocarbon black powder simultaneously, the mixture in the collecting chamber is delivered in two planetary stirring machines again; Second stage is the conventional flow process that stirs, and promptly high-speed stirred is 4 hours, obtains final slurry.
The average grain diameter that adopts the droplet distribution recognizer to measure PVDF solution droplet is 486.9 microns, and the average grain diameter of cobalt acid lithium dust cloud particle is 26.12 microns, and the average grain diameter of carbon black dust cloud particle is 1.77 microns.
Comparative Examples 5
Adopt the raw material identical, adopt common alr mode to make slurry with embodiment 6.Get the final slurry of embodiment 6 and Comparative Examples 5 respectively, adopt the Malvern laser particle analyzer to measure the pulp particle degree respectively, the result is as shown in Figure 6.Can find out that the granularity of embodiment 6 is less than Comparative Examples 5, explain under same stirring condition that the slurry dispersion effect of mist attitude premix slightly is superior to contrast groups.This is because the solvent of anode sizing agent is NMP, and is very good to the wetting effect of cobalt acid lithium powder, and in level preferably, mist attitude premix has some improvement on its basis the dispersion effect of common stirring.
Claims (10)
1. the preparation method of a lithium ion battery electrode sizing agent is characterized in that,
Premix: in hybrid chamber, adopt spray pattern simultaneously liquid material and powder material to be advanced the mist state premix;
Stir: the mixture behind the premix is carried out mechanical agitation, make electrode slurry.
2. the preparation method of lithium ion battery electrode sizing agent according to claim 1 is characterized in that: described powder material comprises at least a in active material powder, conductive agent powder, bonding agent powder and the additive agent powder.
3. the preparation method of lithium ion battery electrode sizing agent according to claim 1; It is characterized in that: described liquid material is any one or the two or more combination in water, alcohol, acetone, N-methyl pyrrolidone, dimethyl formamide, dimethylacetylamide or the dimethyl sulfoxide (DMSO), or is the solution of one or more bonding agents.
4. the preparation method of lithium ion battery electrode sizing agent according to claim 3 is characterized in that: in liquid material, can also add the additive that is used to improve battery processing characteristics, electrical property or security performance in advance.
5. the preparation method of lithium ion battery electrode sizing agent according to claim 1 is characterized in that: said liquid material adopts the turbulent flow mode to contact with powder material.
6. the preparation method of lithium ion battery electrode sizing agent according to claim 5 is characterized in that: said turbulent flow mode is collision type contact or spiral vortex type contact.
7. the preparation method of lithium ion battery electrode sizing agent according to claim 1 is characterized in that: before liquid material spraying and powder material sprinkling, can also carry out the physics pre-treatment of heat, electricity, magnetic to liquid or powder.
8. the preparation method of lithium ion battery electrode sizing agent according to claim 1 is characterized in that: the average diameter of the mist attitude drop that liquid material forms is between 1～500 micron.
9. the preparation method of lithium ion battery electrode sizing agent according to claim 1 is characterized in that: the average grain diameter of the particle that powder material forms is between 0.1～50 micron.
10. the preparation method of lithium ion battery electrode sizing agent according to claim 1, it is characterized in that: the weight proportion of liquid material and powder material is between 98: 2～20: 80.
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| CN103811714A (en) * | 2012-11-09 | 2014-05-21 | 丰田自动车株式会社 | Method for producing aqueous electrode paste and two-shaft kneader |
| CN105470520A (en) * | 2015-12-01 | 2016-04-06 | 东莞市创明电池技术有限公司 | Preparation method of slurry for lithium-ion battery |
| CN107293706A (en) * | 2017-05-10 | 2017-10-24 | 惠州拓邦电气技术有限公司 | Lithium ion battery cathode slurry and its fast preparation method and its negative plate |
| WO2018113486A1 (en) * | 2016-12-22 | 2018-06-28 | 深圳拓邦股份有限公司 | Slurry for lithium-ion battery and preparation method therefor |
| CN108258188A (en) * | 2018-01-12 | 2018-07-06 | 安徽益佳通电池有限公司 | A kind of dry-mixed preparation method of lithium ion battery electrode sizing agent |
| CN108574088A (en) * | 2017-03-10 | 2018-09-25 | 上海兆维科技发展有限公司 | A kind of anode sizing agent and preparation method thereof |
| CN111224059A (en) * | 2018-11-27 | 2020-06-02 | 多氟多化工股份有限公司 | Dispersing method and device for electrode slurry containing carbon nano tubes |
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| CN108258188B (en) * | 2018-01-12 | 2020-08-18 | 安徽益佳通电池有限公司 | Dry-mixing preparation method of lithium ion battery electrode slurry |
| CN111224059A (en) * | 2018-11-27 | 2020-06-02 | 多氟多化工股份有限公司 | Dispersing method and device for electrode slurry containing carbon nano tubes |
| CN111224059B (en) * | 2018-11-27 | 2021-09-24 | 多氟多新材料股份有限公司 | Dispersing method and device for electrode slurry containing carbon nano tubes |
| CN113380973A (en) * | 2021-06-15 | 2021-09-10 | 湖南美尼科技有限公司 | Preparation method of silicon-based negative electrode slurry |
| CN113769633A (en) * | 2021-08-27 | 2021-12-10 | 合肥国轩高科动力能源有限公司 | Lithium ion battery slurry mixing method |
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| CN102386378B (en) | 2016-03-02 |
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